Progress Report

Design of a Characterization Protocol for Carbon-based Fuel Cell Catalyst Supports Sponsored by UTC Power Adam Wentworth Faculty Advisor: Dr. Mark Aindow Industry Advisor: T.T. Cheng-Aindow

Need ,[object Object],[object Object],[object Object]

Specific Objectives ,[object Object],[object Object],[object Object]

Plan of Work ,[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object]

Terminology/Breakdown ,[object Object],[object Object],[object Object],[object Object],Image provided by reference [3].

Raman Spectroscopy ,[object Object],[object Object],http://newton.ex.ac.uk/research/biomedical/optics/images/Raman.jpg

Raman Features ,[object Object],[object Object],[object Object],[object Object],Image from ref [6]. I G I D I A

Curve Fitting Vulcan Ensaco I G I D I A I D I D I G I G I A I A Image from ref [6]. Renishaw Ramascope Micro-Raman spectrometer using iWire software

Preliminary Data (Raman) ,[object Object],[object Object],[object Object],Charts from prior testing done by Dr. Lichun Zhang D

Preliminary Data (Raman) ,[object Object],[object Object]

Peak Shifts ,[object Object],[object Object],Values represent the change in the peak after graphitization process. Ensaco Ketjan Timrex Vulcan Blk Pearl Hyperion G shift ↕ [Intensity] 717.41 144.28 -68.25 656.43 43.77 325.21 D shift ↕ [Intensity] -96.32 -459.58 125.77 -53.87 -98.33 -534.67 G shift ↔ [cm -1 ] -8.22 -13.44 -6.11 -9.04 -0.74 -14.89 D shift ↔ [cm -1 ] -2.2 9.31 -6.06 -4.57 -10.03 -1.23 G width [cm -1 ] -57.14 -37.62 15.2 -62.93 -52.132 -35.36 D width [cm -1 ] -187.57 -74.31 14.01 -168.03 -204.35 -33.66

Crystallite Size vs. I G /I D Ratio ,[object Object],[object Object],[object Object],[object Object],[object Object]

Approximate Crystallite Sizes ,[object Object],[object Object],[object Object],Crystallite Size (Lateral Area) [nm] La = 4.35 I G /I D [nm] *assumes equation is valid. Ensaco Ketjan Timrex Vulcan Blk Pearl Hyperion Nanoblk Acet Blk GlassyCrb Ungraphitized 4.85 4.015 17.23 4.589 4.106 3.975 19.83 5.211 3.201 Graphitized 14.19 11.87 9.487 12.91 6.250 30.05 Growth 9.34 7.860 -7.747 8.330 2.144 26.08

Graphite / Diamond sp 2 hybridized bonding Lattice parameter c = 3.350 Ǻ sp 3 hybridized bonding Lattice parameter a = 3.567 Ǻ Images courtesy of http://cst-www.nrl.navy.mil/lattice/ c a

Preliminary Data (XRD) HOPG (Highly Oriented Pyrolitized Graphite) Ensaco Ensaco - Graphitized

Preliminary Data (XRD) Hyperion Hyperion - Graphitized Printex Electrode ,[object Object],002 100 004 110 Image provided by ref [3]. 002 100 101

[object Object],Preliminary Data (XRD) Timrex Timrex - Graphitized 002 100/101 004 110 006 002 004

XRD Analysis ,[object Object],[object Object],[object Object],Lattice parameter c [Ǻ] before and after graphitization Graphitized Ungraphitized ENSACO KETJAN VULCAN HYP BLKPRL TIMREX HOPG ungraphitized 3.626 3.570 3.570 graphitized 3.457 3.404 3.467 3.539 3.442 3.401 3.356 ungraphitized 3.004 3.501 3.377

XRD Analysis (Linear Regression) ,[object Object],[object Object],Comparison of lattice parameters using Bragg’s Law and linear regression methods. Ensaco Vulcite BlkPearl Timrex HOPG LR1 3.442 3.426 3.448 3.371 3.345 LR2 3.438 3.414 3.45 3.367 3.35 Average (LR) 3.44 3.42 3.449 3.369 3.347 XRD 3.457 3.467 3.442 3.401 3.356 SD (avg+XRD) 0.008 0.023 0.003 0.016 0.004

[object Object],XRD Analysis (Crystallite Size) β – FWHM [radians] K – constant 0.9 λ – wavelength radiation [nm] cos θ – center of peak [radians] L – crystallite size [nm]

Next Step TEM ,[object Object],[object Object],[object Object],[object Object],[object Object],Image provided by reference [3].

Preliminary Data (TEM) Timrex-Graphitized 25KX 50KX 100KX

Preliminary Data (TEM) Timrex-Graphitized ,[object Object],[object Object],200KX 400KX 400KX

Preliminary Data (TEM) Timrex-Ungraphitized ,[object Object],25KX 50KX 100KX

Preliminary Data (TEM) Timrex-Ungraphitized ,[object Object],[object Object],400KX 400KX

[object Object],[object Object],[object Object],[object Object],[object Object],Next Step Thermogravimetric Analysis http://www.msel.nist.gov/Nanotube2/Practice%20Guide_Section%202_TGA.pdf

Meaning of values ,[object Object],[object Object],[object Object],[object Object],http://www.msel.nist.gov/Nanotube2/Practice%20Guide_Section%202_TGA.pdf

[object Object],[object Object],Next Step Gas Adsorption

Constraints ,[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object]

Characterization Criteria ,[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object]

Summary ,[object Object],[object Object],[object Object],[object Object]

References ,[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object]

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